深圳大学学报（理工版）
深圳大學學報（理工版）
심수대학학보（리공판）
Journal of Shenzhen University(Science & Engineering)
2015年
5期
465-472
,共8页
巫剑波%秦草坪%袁秋华%郭志威%刘家裕%邓庆威%张培新
巫劍波%秦草坪%袁鞦華%郭誌威%劉傢裕%鄧慶威%張培新
무검파%진초평%원추화%곽지위%류가유%산경위%장배신
无机仿生材料%羟基磷灰石%湿化学法%水浴合成%常温合成%高结晶度和纯度%晶体表征
無機倣生材料%羥基燐灰石%濕化學法%水浴閤成%常溫閤成%高結晶度和純度%晶體錶徵
무궤방생재료%간기린회석%습화학법%수욕합성%상온합성%고결정도화순도%정체표정
inorganic biomimetic materials%hydroxyapatite%wet chemistry method%water bath synthesis%room temperature synthesis%high crystallinity and purity%crystal characterization
采用湿化学法通过两种方案合成羟基磷灰石 ( hydroxyapatite, HA ) 晶体, 一种方案是以Ca (NO3)2·4H2O和Na2HPO4 作为原料, 加入NaOH溶液调节pH值在10. 5 ~11. 0 之间, 不添加分散剂,在40 ℃水浴条件下合成羟基磷灰石; 另一方案是在室温下 ( 25 ℃) 进行, 在其他条件不变的情况下, 以CaCl2·2H2 O为钙源、 乙醇胺作为分散剂合成羟基磷灰石. 将两种方案合成的样品分别通过X射线衍射( X-ray diffraction, XRD)、 傅里叶变换红外光谱 ( Fourier transform infrared spectroscopy, FTIR)、 扫描电子显微镜 ( scanning electron microscopy, SEM)、 X射线能量色散仪 ( energy-dispersive X-ray spectroscopy, EDX)、热重-差热分析和X射线光电子能谱 ( X-ray photoelectron spectroscopy, XPS) 进行表征. XRD和FTIR结果显示, 合成的两种HA粉末都具有较高结晶度和纯度. SEM分析表明, 第1 种方案可合成直径为30 ~50 nm, 长50~150 nm的棒状晶体; 第2种方案则可制备粒径约100~150 nm的球状 (或椭球状) 晶体. 热分析表明, 所制备的HA在1 000 ℃范围内有显著的热稳定性. XPS和EDX分析则证实HA由Ca、 P和O等元素组成, 两种方案中钙和磷的摩尔比分别是1. 60和1. 63 .
採用濕化學法通過兩種方案閤成羥基燐灰石 ( hydroxyapatite, HA ) 晶體, 一種方案是以Ca (NO3)2·4H2O和Na2HPO4 作為原料, 加入NaOH溶液調節pH值在10. 5 ~11. 0 之間, 不添加分散劑,在40 ℃水浴條件下閤成羥基燐灰石; 另一方案是在室溫下 ( 25 ℃) 進行, 在其他條件不變的情況下, 以CaCl2·2H2 O為鈣源、 乙醇胺作為分散劑閤成羥基燐灰石. 將兩種方案閤成的樣品分彆通過X射線衍射( X-ray diffraction, XRD)、 傅裏葉變換紅外光譜 ( Fourier transform infrared spectroscopy, FTIR)、 掃描電子顯微鏡 ( scanning electron microscopy, SEM)、 X射線能量色散儀 ( energy-dispersive X-ray spectroscopy, EDX)、熱重-差熱分析和X射線光電子能譜 ( X-ray photoelectron spectroscopy, XPS) 進行錶徵. XRD和FTIR結果顯示, 閤成的兩種HA粉末都具有較高結晶度和純度. SEM分析錶明, 第1 種方案可閤成直徑為30 ~50 nm, 長50~150 nm的棒狀晶體; 第2種方案則可製備粒徑約100~150 nm的毬狀 (或橢毬狀) 晶體. 熱分析錶明, 所製備的HA在1 000 ℃範圍內有顯著的熱穩定性. XPS和EDX分析則證實HA由Ca、 P和O等元素組成, 兩種方案中鈣和燐的摩爾比分彆是1. 60和1. 63 .
채용습화학법통과량충방안합성간기린회석 ( hydroxyapatite, HA ) 정체, 일충방안시이Ca (NO3)2·4H2O화Na2HPO4 작위원료, 가입NaOH용액조절pH치재10. 5 ~11. 0 지간, 불첨가분산제,재40 ℃수욕조건하합성간기린회석; 령일방안시재실온하 ( 25 ℃) 진행, 재기타조건불변적정황하, 이CaCl2·2H2 O위개원、 을순알작위분산제합성간기린회석. 장량충방안합성적양품분별통과X사선연사( X-ray diffraction, XRD)、 부리협변환홍외광보 ( Fourier transform infrared spectroscopy, FTIR)、 소묘전자현미경 ( scanning electron microscopy, SEM)、 X사선능량색산의 ( energy-dispersive X-ray spectroscopy, EDX)、열중-차열분석화X사선광전자능보 ( X-ray photoelectron spectroscopy, XPS) 진행표정. XRD화FTIR결과현시, 합성적량충HA분말도구유교고결정도화순도. SEM분석표명, 제1 충방안가합성직경위30 ~50 nm, 장50~150 nm적봉상정체; 제2충방안칙가제비립경약100~150 nm적구상 (혹타구상) 정체. 열분석표명, 소제비적HA재1 000 ℃범위내유현저적열은정성. XPS화EDX분석칙증실HA유Ca、 P화O등원소조성, 량충방안중개화린적마이비분별시1. 60화1. 63 .
Hydroxyapatite ( HA) crystals were synthesized by two new wet chemistry methods. The first method was carried out by using calcium nitrate tetrahydrate and disodium hydrogen phosphate as starting materials and adding sodium hydroxide to ensure the pH value ranging from 10. 5 to 11. 0 under 40 ℃ water bath with no dispersant. For the other method, hydroxyapatite was synthesized at room temperature (25 ℃) with calcium chloride dehydrate as calcium source and ethanolamine as dispersing agent, while other conditions remained the same as those in the first method. The obtained samples were characterized by X-ray diffraction ( XRD ) , fourier transform infrared spectroscopy ( FTIR ) , scanning electron microscopy ( SEM ) coupled with energy-dispersive X-ray spectroscopy ( EDX) , thermogravimetric analysis-differential thermal analysis ( TG-DTA) , and X-ray photoelectron spectroscopy (XPS), respectively. The XRD and FTIR results exhibit that the synthesized HA has a high crystallinity and purity.The SEM images reveal that rod-like HA crystals with a diameter of 30-50 nm and a length of 50-150 nm are formed by using the first method, while spherical or ellipsoidal HA crystals with a diameter of 100-150 nm around can be obtained through the second method. The thermal analysis shows that the synthesized HA has a remarkable heat stability up to 1 000 ℃,and the XPS and EDX studies indicate that HA samples are predominantly composed of elements including calcium (Ca), phosphorous (P), oxygen (O), etc. The ratios of Ca and P of HA samples in the first and the second methods are equal to 1. 60 and 1. 63, respectively.
